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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
  • C08F212/02—Monomers containing only one unsaturated aliphatic radical
  • C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
  • C08F212/06—Hydrocarbons
  • C08F212/08—Styrene
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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
  • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
  • C08F220/04—Acids; Metal salts or ammonium salts thereof
  • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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  • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
  • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
  • C08F220/10—Esters
  • C08F220/12—Esters of monohydric alcohols or phenols
  • C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
  • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
  • C08F220/10—Esters
  • C08F220/12—Esters of monohydric alcohols or phenols
  • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
  • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
  • C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
  • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
  • C08F220/10—Esters
  • C08F220/34—Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
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  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
  • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
  • C08F220/10—Esters
  • C08F220/38—Esters containing sulfur
  • C08F220/382—Esters containing sulfur and containing oxygen, e.g. 2-sulfoethyl (meth)acrylate
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
  • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
  • C08F220/10—Esters
  • C08F220/40—Esters of unsaturated alcohols, e.g. allyl (meth)acrylate
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  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
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  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
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  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
  • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
  • C09C1/36—Compounds of titanium
  • C09C1/3607—Titanium dioxide
  • C09C1/3676—Treatment with macro-molecular organic compounds
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  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
  • C09D133/04—Homopolymers or copolymers of esters
  • C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
  • C09D133/04—Homopolymers or copolymers of esters
  • C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
  • C09D133/08—Homopolymers or copolymers of acrylic acid esters
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  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
  • C09D151/10—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to inorganic materials
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  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
  • C09D7/40—Additives
  • C09D7/42—Gloss-reducing agents
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  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
  • C09D7/40—Additives
  • C09D7/60—Additives non-macromolecular
  • C09D7/61—Additives non-macromolecular inorganic
  • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
  • C09D7/40—Additives
  • C09D7/65—Additives macromolecular
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  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
  • C09D7/40—Additives
  • C09D7/66—Additives characterised by particle size
  • C09D7/69—Particle size larger than 1000 nm
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K3/00—Use of inorganic substances as compounding ingredients
  • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
  • C08K3/20—Oxides; Hydroxides
  • C08K3/22—Oxides; Hydroxides of metals
  • C08K2003/2237—Oxides; Hydroxides of metals of titanium
  • C08K2003/2241—Titanium dioxide
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K9/00—Use of pretreated ingredients
  • C08K9/10—Encapsulated ingredients

Definitions

• the present invention relates to a low sheen paint composition with effective opacity.
• Control of gloss is critical in the design and application of protective and/or decorative low sheen paints.
• matting agents also known as dullers, which are either inorganic particles, such as silica or calcium carbonate particles, or organic particles, such as polyurethane dispersions or urea-formaldehyde resins that function by roughening the surface of the film. While effective at reducing gloss, these dullers result in a significant degree of light scattering, both forward scatter and backscatter, and in internal and external reflection. Such uncontrolled interaction of light with the duller particles can cause graying, haziness, cloudiness, loss of color intensity and a washed-out appearance of the coated article. Furthermore, such duller particles often disrupt film integrity and can lead to loss of key film properties such as water and abrasion resistance, and flexibility. Still further, such duller particles tend to polish or burnish after rubbing, leading to an increase in gloss.
• the present invention provides an aqueous paint composition comprising by dry weight based on total dry weight of the pigment composition, from 11% to 35% of a polymeric duller of (co)polymeric particles having an average diameter of from 1 to 20 ⁇ m, and from 25% to 70% of titanium dioxide particles, wherein from 50% to 100% of the titanium dioxide particles are encapsulated by (co)polymeric particles.
• (co)polymeric refers to polymeric or copolymeric.
• the present invention provides an aqueous paint composition
• an aqueous paint composition comprising by dry weight based on total dry weight of the paint composition, from 11% to 35%, preferably from 12% to 25%, and more preferably from 13% to 22%, a polymeric duller of (co)polymeric particles having an average diameter of from 1 to 20 ⁇ m, preferably from 2 to 10 ⁇ m, and more preferably from 3 to 7 ⁇ m; and from 25% to 70%, preferably from 28% to 55%, and more preferably from 30% to 40%, titanium dioxide particles. From 50% to 100%, preferably from 60% to 100%, and more preferably from 70% to 100% by dry weight based on total dry weight of the titanium dioxide particles are encapsulated by polymer shell of (co)polymeric particles.
• the aqueous paint composition further comprises a binder component comprising film forming organic polymer of (co)polymeric particles.
• the (co)polymeric particles of the present invention comprise at least one polymerized ethylenically unsaturated nonionic monomer.
• ethylenically unsaturated nonionic monomers include alkyl esters of (methyl) acrylic acids such as methyl acrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, decyl acrylate, lauryl acrylate, methyl methacrylate, butyl methacrylate, isodecyl methacrylate, lauryl methacrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, and mixtures thereof; (meth)acrylonitrile; (meth)acrylamide; amino-functional and ureido-functional monomers such as hydroxyethyl ethylene urea methacrylate; monomers bearing acetoacetate-functional groups such as acetoacetoxyethyl methacrylate (AAEM); monomers bearing carbonyl-containing groups such as diacetone acrylamide (DAAM); ethylenically unsaturated monomers
• the ethylenically unsaturated nonionic monomers are selected from methyl methacrylate, ethyl acrylate, butyl acrylate, 2-ethylhexyl acrylate, styrene, vinyl acetate, vinyl butyrate, and mixtures thereof.
• the (co)polymeric particles may further comprise less than 10%, preferably less than 5%, and more preferably less than 2.5% by dry weight based on total dry weight of the (co)polymeric particles, of a stabilizer monomer.
• a stabilizer monomer include sodium styrene sulfonate (SSS), sodium vinyl sulfonate (SVS), 2-acrylamido-2-methylpropanesulfonic acid (AMPS), acrylamide (AM), acrylic acid (AA), methylacrylic acid (MAA), and itaconic acid (IA).
• the (co)polymeric particles of the polymeric duller have a minimum film forming temperature (MFFT) of above 50° C., and an average diameter of from 1 to 20 ⁇ m.
• MFFT film forming temperature
• the (co)polymeric particles of the polymer shell encapsulating the titanium dioxide particles have an MFFT of from ⁇ 50 to 100° C., and an average diameter of from 200 to 800 nm.
• the (co)polymeric particles of the film forming organic polymer of the binder component have an MFFT of from ⁇ 50 to 100° C., and an average diameter of from 50 to 500 nm.
• MFFT is the lowest temperature at which (co)polymeric particles or solid portion of an aqueous polymer dispersion (also called latex or emulsion) self coalesces in the semi dry state to form a continuous polymer film, which in turn acts as a binder for the rest of the solids in the paint film.
• aqueous polymer dispersion also called latex or emulsion
• the polymer film is formed.
• temperatures below its MFFT the polymer cannot coalesce to form a continuous film.
• titanium dioxide (TiO 2 ) particles can be used in the paint composition of the present invention.
• Commercially available titanium dioxide particles include TI-PURETM R-706 and TI-PURE R-902+ from DuPont, TIONATM 595 of Millennium Inorganic Chemicals, TIOXIDETM TR92 from Huntsman Corporation, LOMONTM R-996 and LOMON LR-997 of LOMON Corporation, BILLIONTM BLR-688 and BILLION BLR-699 from Henan Billions Chemical co., Ltd., DOGUIDETM SR-237 from Shandong Doguide Group Co., Ltd., NTR-606 from Ningbo Xinfu Titanium Dioxide Co., Ltd., and R-2195 and R-2295 from Dawn Group.
• the titanium dioxide particles are selected from TI-PURE R-706 and TI-PURE R-902+ available from DuPont.
• the encapsulation of the polymer shell of (co)polymeric particles on the surface of the titanium dioxide particles can be achieved by polymerization processes.
• the polymerization processes can be any methods known in the art, including emulsion polymerization, mini-emulsion polymerization, and mechanical dispersing technology.
• the paint composition may further comprise other pigments or extenders.
• pigment refers to a particulate inorganic material which is capable of materially contributing to the opacity or hiding capability of a paint. Pigments typically have a refractive index of equal to or greater than 1.8 and include zinc oxide, zinc sulfide, barium sulfate, and barium carbonate. For the purpose of clarity, titanium dioxide particles of the present invention are not included in the “pigment” of the present invention.
• the term “extender” refers to a particulate inorganic materials having a refractive index of less than or equal to 1.8 and greater than 1.3 and include calcium carbonate, aluminium oxide (Al 2 O 3 ), clay, calcium sulfate, aluminosilicate, silicate, zeolite, mica, diatomaceous earth, solid or hollow glass, and ceramic bead.
• the paint composition may optionally contain solid or hollow polymeric particles having a Tg of greater than 60° C., such polymeric particles are classified as extenders for purposes of pigment volume concentration (PVC) calculations herein.
• PVC pigment volume concentration
• the solid polymeric particles have particle sizes of from 1 to 50 microns, and preferably from 5 to 20 microns.
• a suitable example of the polymeric particles is ROPAQUETM Ultra E opaque polymer commercially available from The Dow Chemical Company.
• the polymeric particles of the present invention are different from the first or the second polymer of the present invention. Calcium carbonate, clay, mica, and aluminium oxide (Al 2 O 3 ) are preferred extenders.
• the paint composition has a PVC of from 10% to 75%, and preferably from 20% to 70%.
• the preparation of the paint composition can be well-known methods of the art and involves the process of admixing appropriate paint ingredients in the indicated proportions to provide a paint as well as a final dry paint film with the desired properties.
• the paint composition may be applied by conventional application methods such as brushing, roller application, and spraying methods such as air-atomized spray, air-assisted spray, airless spray, high volume low pressure spray, and air-assisted airless spray.
• Suitable substrates for paint application include concrete, cement board, medium-density fiberboard (MDF) and particle board, gypsum board, wood, stone, metal, plastics, wall paper and textile, etc.
• MDF medium-density fiberboard
• gypsum board wood, stone, metal, plastics, wall paper and textile, etc.
• all the substrates are pre-primed by waterborne or solvent-borne primers.
• Contrast ratio of dry paint was determined by a BYK-Gardner 6850 Color-Guide Plus Spectrophotometer. Contrast ratio is a test method for the opacity of paint film, Y values of paint film were tested separately in the white chart (Y w ) and black chart (Y b ). Contrast ratio was defined as Y b /Y w . The higher the contrast ratio, the better the opacity.
• Form P121-10N Leneta Scrub Test Panels were coated by paint compositions followed by being dried for 7 days in a CTR (25° C., 50% R.H.). Hydrophilic stains including red wine, coffee, black tea, green tea, and ink were applied by placing cheese clothes saturated with the corresponding stains on the surface across the paint film and were allowed for staying for 2 hours. Prior to the stain resistance test, Y value of each paint film (labeled as Y0) was tested by a BYK-Gardner 6850 Color-Guide Plus Spectrophotometer. Excessive liquid stains were wiped off with a paper towel or cheese cloth.
• the stain resistance test was conducted on a JTX-architecture paint scrub machine of Shanghai Xiandai Environment Engineering Technique Co., Ltd. with a 3MTM commercial sponge saturated with 1% OMOTM wash powder solution. Each paint film was washed for 100 cycles. Before reading, the panels were rinsed with water followed by being completely dried at room temperature. Y value of the paint film surface area which was covered by stain mark was tested and labeled as Y1.
• the stain resistance ratio was defined as R, and
• Stain resistance performance for each stain was evaluated by following the standard described in Table 1.
• a 250 ml flask equipped with a magnetic stirrer, an N 2 -inlet, a reflux condenser, a heating mantel, and a thermocouple was charged with 20 g of SEM, 4 g of DMAEMA, 10 g of BA, 16 g of MMA, 1.1 g of n-DDM, 0.5 g of AIBN, and 100 g of n-propanol.
• the flask was purged with N 2 , and heated to 80° C. for 3 hours. The temperature was then raised to 93° C., and 0.25 g of AIBN in 2.0 g n-propanol was added. The temperature was held at 93° C. for 1 hour; then the flask was cooled to room temperature.
• the product was poured into 100 ml of hexane, and was dried. The dried product was dissolved in sufficient water and NH 3 to make a 21.3% solution at pH 5.0 to prepare a dispersant polymer.
• a steel grind pot was charged with 31.7 g of the dispersant polymer and 95.2 g of water. 450 g TI-PURETM R-706 TiO 2 was added slowly while grinding at 2000 rpm using a Model 50 Lab Dispersator equipped with a disk blade. The mixture was ground for 20 min, and then an additional 11.3 g of water was added to make a 76.5% TI-PURE R-706 TiO 2 slurry.
• a 1 gallon four-neck round-bottom flask equipped with a paddle stirrer, an N 2 -inlet condenser, a heating mantel, and a thermocouple was charged with 1816 g of the slurry along with a solution of 13.81 g DS-4 (23% solids) in 251.05 g DI water.
• the flask was purged with N 2 , and heated to 30° C. Then 50 g 0.1% iron sulfate and 4 g 1% EDTA were added into the reactor.
• co-feed #1 consisting of 2 g t-BHP dissolved in 110.53 g DI water and co-feed #2 consisting of 8.28 g IAA dissolved in 96.25 g DI water were fed to the reactor.
• a first monomer emulsion (ME1) prepared previously by mixing 56.52 g DI water, 6.9 g DS-4, and 261.67 g monomers (45.6% BA, 53.4% MMA and 1.0% MAA) was fed to the reactor.
• a second monomer emulsion prepared by mixing 269.5 g DI water, 20.71 g DS-4, and 779.5 g monomers (45.6% BA, 53.4% MMA and 1.0% MAA) was fed to the reactor. Reaction continued for another 20 min. The contents of the reactor were then cooled to room temperature, followed by feeding 84 g NaOH solution (6% solids) in 40 min. Small amounts of gel were filtered by a 100 mesh filter. The remainder was the dispersion of polymer encapsulated titanium dioxide particles. The dispersion comprised 33% titanium dioxide particles, 26% (co)polymeric particles, and water.
• a reactor equipped with stirrer and condenser and blanketed with nitrogen was charged with 208 g of DI water and 0.38 g of sodium carbonate, and was heated to 82° C. 15% of mixture 1 (MIX1) of 98 g of BA, 0.25 g of butylenes glycol diacrylate, 2.0 g of ALMA, 4.0 g of 10% DS-4 solution, and 40 g of DI water, and 25% of mixture 2 (MIX2) of 0.063 g of potassium persulfate, and 35 g of DI water, were added to the reactor contents. The temperature was maintained at 82° C.
• MIX1 mixture 1
• MIX2 mixture 2
• the reaction mixture was stirred for 1 hour, after which the remaining MIX1 and MIX2 were metered in to the reactor, with stirring, over a period of 90 minutes. Stirring was continued at 82° C. for 2 hours, after which the reactor contents were cooled to room temperature.
• the resulting mixture was a (co)polymeric particles emulsion having an average diameter of 0.2 ⁇ m as measured by a NanoBrook 90Plus Zeta Particle Size Analyzer from Brookhaven Instruments Company.
• MIX3 mixture 3 of 35 g 0.2 ⁇ m average diameter polymeric particles emulsion prepared according to above process (as seed particles), 0.081 g sodium carbonate and 185.0 g DI water was added to the reactor and heated to 88° C. with stirring.
• MIX4 consisting of 82.0 g BA, 18.0 g STY, 2.5 g 10% DS-4 solution and 32.0 g DI water
• MIX5 consisting of 19.0 g 1-hexanethiol
• MIX6 consisting of 0.11 g potassium persulfate dissolved in 18.0 g DI water
• the reactor contents were cooled to 65° C., a mixture 7 (MIX7) consisting of 0.18 g t-BHP dissolved in 3.7 g DI water and 4.1 g 3% SFS solution were added, and the reactor contents were maintained at 65° C., with stirring, for 1 hour, after which the reactor contents were cooled to room temperature.
• the resulting mixture was a (co)polymeric particles emulsion having an average diameter of 0.5 ⁇ m as measured by the NanoBrook 90Plus Zeta Particle Size Analyzer.
• MIX8 mixture 8 consisting of 3.7 g 0.5 ⁇ m average diameter polymeric particles emulsion prepared by above process (as seed particles) and 1830 g DI water, and then heated to 92° C.
• MIX9 consisting of 9.0 g 23% DS-4 solution, 556.0 g BA, 23 g ALMA and 248 g DI water
• MIX10 mixture 10
• MIX9 was then slowly fed into the reactor over one hour. With the reactor contents at 64° C., MIX10 was added as a shot to start the reaction which was complete about 1.5 hours later.
• the resulting mixture was cooled to room temperature and analyzed by examined by optical microscopy and a Coulter Counter.
• the resulting mixture was cooled to room temperature and analyzed by an optical microscopy.
• the resulting mixture was the dispersion of polymeric duller of (co)polymeric particles having an average diameter of 5 m.
• Comparative Paints 1 and 2 (Comp. 1 or 2), and Paints 1, 2, and 3 (Paint 1, 2, or 3) were prepared according to the procedure of Table 2.
• the Grind ingredients were mixed using a high speed Cowles disperser.
• the Let-down ingredients were added using a conventional lab mixer.
• Comparative Paint 2 did not comprise enough polymeric duller (less than required 11% by dry weight based on total dry weight of the paint composition), compared to 12% of Paint 2, therefore, showed very poorer glosses at respectively 20, 60 and 85 degree geometry (2.5/13.4/39.8) compared to those of Paint 2 (1.6/5.9/19.7).
• Comparative Paint 1 did not comprise polymer shell encapsulated titanium dioxide particles, and showed a poorer opacity as indicated by contrast ratio compared to Paints 1 and 3. Its stain resistance is also poorer. This result indicated the critical role played by the polymer shell encapsulation of titanium dioxide particles with (co)polymeric particles in providing paints with satisfactory opacity and stain resistance.

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